REPORT FOR
A New Analytical
Feature
MANAGEMENT
Last month w e set the scene for our series, "Report for Management," with an over-all look a t the place of the analytical department in Chas. Pfizer & Co., Inc. Our author was John E. McKeen, the company's president and chairman of the b o a r d . He told us how important analysis is to quality control, to the development of new products, and to the control of plant processes. He stressed the importance of analysis in effective research programs. For this month's installment w e a r e fortunate, therefore, in having a closer look at the research side by Jesse W . Stillman whose extensive experience with Du Pont gives him a broad insight into the relationship of analysis to research. In succeeding installments other top-flight authorities will discuss the relationship of the analytical department to production, sales, purchasing, product development, and other phases of operations in the modern chemical process industries. —The Editors
JESSE W . S T I L L M A N Supervisor, Physical and Analytical Division, Chemical E. I. du Pont de Nemours & Co., Inc., Wilmington, Del.
Department,
Supervising the Analytical Research Laboratory I HIS ARTICLE will be devoted to the organization and administration of a research analytical laboratory. Many of the points emphasized, however, will apply as well to the production analytical laboratory. The demands made upon the analytical laboratory have been increasing in complexity in recent years since the research chemist has required more precise information about his samples. In the field of organic analysis, for example, a report of the composition in terms of the chemical elements present in most cases is inadequate. Information is required as to how the elements are arranged in groups and where these groups are located in the molecule. As a result, the whole
approach to analytical chemistry has been changed. Chemical methods that yield incomplete information have been supplemented by methods for determining physical properties that are characteristic of a particular compound. Similarly, in the field of inorganic analysis, the so-called "less familiar" elements are now regularly determined. Likewise, elements t h a t are difficult to separate by the customary procedures must be determined in mixtures. This presents a challenge to the analytical chemist and requires that he be backed up by an organization providing him with the necessaryfacilities, tools, and direction. I n planning for or reviewing the organization of a research analytical laboratory, certain factors must be
V O L U M E 2 7, N O . 12, D E C E M B E R
1955
taken into consideration. These include: • Personnel • Laboratory arrangement and facilities • Equipment • Organization and administration Supervision Safety Routing and follow-up on samples Records and reports Research Each of these topics will be discussed separately. Personnel
The effectiveness of any laboratory depends upon the caliber of its tech9A
REPORT FOR M A N A G E M E N T
nical staff and, therefore, careful thought should be given to the recruiting of this staff. Candidates should have a broad training in all fields of chemistry because their work will involve the application of the various branches. Since many of the approaches they will use will also involve physics, courses in this field will be very helpful. Basic in their training, of course, will be some specialization in analytical chemistry. This will supply information and training on how to apply basic chemical knowledge to an analytical problem, which can be summarized by calling it the development of an analytical point of view. Since the analytical chemist is, in effect, a member of the research team, he must keep an open mind and must show initiative in being ready to take the best course of action required to provide the information which the research chemist needs. For the more repetitive and standardized procedures, nontechnical personnel can be trained but they should work under the close direction of a technical person. Requirements for nontechnical personnel are t h a t they be keen and alert, willing to follow instructions exactly, and dexterous in the ordinary laboratory operations after suitable training. Graduation from high school is a minimum requirement and some college training is an advantage. Laboratory Arrangement a n d Facilities
For efficient operation, careful consideration should be given to the laboratory layout to avoid lost motion in the conduct of the work. For example, today it is considered the best practice to have an analytical balance located near the individual work area instead of in a central location or in a separate room located some distance away. There are some special requirements of an analytical laboratory, which make the standard laboratory design for research purposes inconvenient. Among these are the provision for the permanent location of apparatus assemblies such as thermostat baths, batteries of reflux condensers for running saponification numbers, etc. Some of the large instruments found regularly in the analytical laboratory such as the emission spectrograph require sufficient space to provide access to the instrument from all sides. It is hardly necessary to remark that many of the modern instruments, in order to function properly, require that the laboratory be air conditioned
at least during the hot, humid months. It is poor economy to expect the analyst to do good work in cramped or poorly equipped quarters. Equipment
There are available for the use of the analytical chemist a variety of instruments ranging in complexity from a simple titrator to a mass spectrometer. These are tools that simplify the task of the analyst or extend the range or sensitivity of the methods of analysis. If, for example, an automatic titrator will make it possible for an analyst to turn out more work in less time, its use should be recommended. By this means, results will be available in shorter time and at less cost. In considering whether to buy such an instrument, it should be kept in mind that somewhat more than one third of the cost of the analysis is in the salary of the analytical chemist. The saving of his time may pay for the instrument or other special equipment in a reasonable period. Other more complicated instruments, such as the infrared spectrometer or x-ray diffractometer, are designed to provide specialized information, and because of the comparatively high cost, decisions have to be made as to whether the information supplied by them will be sufficiently useful in solving analytical problems at hand and whether there will be sufficient work to keep the instrument busy most of the time. In some cases information which is essential for the characterization of a research product can be obtained only by one of these instruments. The importance of the research will then dictate whether or not the purchase of the instrument is justified. It should be pointed out that the operation of the instrument can be learned readily in most cases after a period of training, but understanding the design of the instrument and interpreting the results obtained from it require technical knowledge and experience. In other words, the instrument should be looked upon as a tool to increase the effectiveness of the chemist in solving his problems, and it cannot be considered as a substitute for or a displacement of technical personnel. Organization and Administration
In order to handle the steady flow of diverse samples which come out of research programs and to ensure that the research chemist is given the data he requires, at least as far as this is
V O L U M E 2 7, NO. 12, DECEMBER
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REPORT FOR MANAGEMENT possible, the analytical laboratory must have a carefully planned organization. Supervision. The function here is to provide a basic philosophy for organization, so that staff members will be stimulated to put forth their best efforts to cooperate fully with the sender of the sample in providing him with the data he needs however unusual or unreasonable the request may appear to be. Another function is to provide technical knowledge and advice to assist members of the staff in their work. Of course, supervision will assign the work to individual members of the staff and will be responsible for seeing that the work is properly carried out. I t will be the responsibility of supervision to make recommendations for improvement in the operation of the work under their direction and to see that proper steps are taken to correct such situations as the failure of a particular method to work for a particular sample, which may involve the presence of an unusual combination of elements, or to develop a new method when at present it is impossible to analyze a certain sample. Because of the complexity of the problems that he will have to handle, the supervisor should have graduate training or the equivalent in wide experience in the field in which he is to work. A brief description of the organization of the physical and analytical division of the chemical department at the Du Pont Experimental Station will serve to illustrate some of the principles which have been discussed. The division has on its staff 42 technical employees, 38 nontechnical laboratory employees, and 6 clerical employees. General administration is handled by a division head and two assistant division heads who are responsible for the over-all operation of the division. The division is organized in four sections, each under the direction of a supervisor. The sections include 10 to 12 technical persons and handle types of work that are somewhat related. The number of 10 to 12 persons is about as many as one supervisor can direct and keep in close contact with the work being done by them. The supervisor of each section assigns work to the individual chemists in his section, suggests possible procedures to use, and follows the progress of the work. To coordinate the work of the four sections, a meeting of the four section supervisors with the three division heads is held weekly. At this meeting each supervisor reports on the status of the work in his section. Any unusual problems are presented and 12 A
discussed, and suggestions are made as to possible methods of solution. If work has been delayed by an overload on a particular chemist or group, the possibility of transferring a chemist from another assignment which may be in a different section is considered, and a decision made. Safety. In the course of his work the analytical chemist handles many materials, which are toxic when they are breathed or come in contact with the skin. It is the safest procedure to consider any compound toxic and to handle it accordingly. Not only should the usual precautions be taken, such as the use of hoods, adequate ventilation, etc., but provision should be made for unusual situations, such as apparatus leaks or breakage, spills, etc. Responsibility for safe practices should be an integral part of the job of every staff member whether supervisor, technical, or nontechnical. To promote individual responsibility the laboratory rooms should be inspected for safety hazards regularly by committees, made up of both technical and nontechnical employees. Membership on these inspection committees should be rotated so that each employee serves a turn as committee member. Inspections should be conducted systematically, as, for example, looking for broken glassware one time and for electrical hazards another. The safety inspection committees should report to group safety meetings where also topics concerned with safety can be presented and discussed. Routing and Follow-Up on Samples. To facilitate handling, samples for analysis should be submitted to a central receiving office. When received, the sample should be given a serial number which identifies it from that time on. It is important that the system for handling samples be designed to expedite and not to hinder the work of the analyst. The system should be such that it can be administered by the clerical staff, and the analytical chemist should not have to spend time searching for the sample when he is ready for it. In our physical and analytical division, the sample takes the following route: After being given a serial number, the sample is placed on the incoming sample shelf in the order of its serial number. When an analytical chemist is given an assignment, he is given an analytical report form (to be described later), which shows the serial number of the sample. When he is ready to analyze this sample, he finds the sample on the incoming sample shelf and weighs out the portion that he needs for his analysis. If there
are other determinations to be made, he returns the sample immediately to the incoming sample shelf in its proper location according to serial number. When the last chemist has finished with the sample, he places it on one of the outgoing sample shelves. There are five outgoing sample shelves, one designated for each of the working days in the week. Samples are retained for one week in case any questions arise about the analysis or in case repeat determinations are required. Early on the following Monday morning, to use this day as an example again, a clerk removes all of the samples from the Monday shelf and marks them for return to the senders by the delivery service. This leaves the shelf empty again to receive samples completed on that day. Of course, special handling has to be given to samples which may decompose on standing, and storage in the refrigerator may be substituted for the open shelf. Records and Reports. Analytical data are important in establishing that a compound has actually been produced and are frequently used in supporting a patent. The data should be recorded systematically and in such form that at any later date reference can be made to them. The original data obtained as the analysis progresses should be recorded in permanent form. Figures should not be jotted down on scraps of paper with the intention of transferring them later to a permanent notebook or report. In our opinion, a loose-leaf report is most convenient and if the system is properly administered, the reports can be protected so that the data will have legal standing in court. A complete description of the analytical record system used in the Du Pont polychemicals department was described in an article by Hale and Stillman [ANAL. CHBM., 24, 143 (1952)].
More recently, a somewhat different system has been described by Schaefermeyer and Smith [ANAL. CHBM., 27,
1040 (1955)]. The record system used in the physical and analytical division of the Du Pont chemical department is similar to that described by Hale and Stillman and will be reviewed briefly. The analytical report form is 63/4 by 33/4 inches. The forms are supplied in packs with sheets of one-trip carbon paper interleaved. The upper half of the form has spaces for a description of the sample, serial number, date of receipt, the name of the sender, and the account to which the cost of the work is to be charged. The lower half of the form is used to report the results of the analysis. ANALYTICAL
CHEMISTRY
REPORT FOR MANAGEMENT When a sample is received, the clerk takes a pack of report forms made up of two white forms and several colored forms and types the infor mation taken from the sample label on the upper half of the form. Si multaneously, by means of carbon paper the same information is typed on a Keysort index card. A typical combination of forms for a case where three different determinations are to be made would be two white, one green, and three yellow forms. The original white form is kept in the records office until the analysis is completed. The second white form together with the Keysort card is placed in a file in the order of the serial number of the sample. One yellow form is given to each of the three chemists who will be working on the sample. The green form is re tained by the supervisor to indicate work that is in progress in his section. The analyst records on the back of his yellow sheet all data that he obtains, such as weights, buret readings, normality of solutions used, and the necessary calculations. When he ob tains the final result, he enters it on the lower half of the front of the yellow sheet. He then goes to the file mentioned above and enters his result on the lower half of the front of the second white copy carrying the same serial number. After the last result has been obtained, the three yellow copies are stapled to the white copy, and the report of the analysis is complete. The clerk takes the original white copy, with the same serial number, which has been retained in the records office, and types on it the results which have been entered on the second white copy by the analysts. The original white copy now goes to the sender of the sample as a report, and the second white copy with data attached is filed according to serial number.
is already typed on the card. By suitable sorting techniques the cards can be classified easily by the categories for which they are punched and when a card is selected, the serial number on it will serve to locate the correspond ing analytical report. For efficient operation the super visor needs to know the trends in total workload, the demands for particular types of determinations and, of course, the costs of laboratory operation. It may be important to know the number of samples being received from each of several sources, such as different departments. In formation of this sort can be obtained from the Keysort cards. It is a good plan for the supervisor to keep run ning curves for any of these data which may be important to him. Such summarized information will be helpful in forecasting future needs for space or personnel. Research. Analytical procedures do not remain static but require constant improvement and change. A research program is required which will provide for the evaluation of new developments which are reported in the literature and for supplying new or revised methods to meet specific needs of the analytical laboratory.
The Keysort card, which was barely mentioned, is used for two pur poses. First, as indicated above, it is placed in a file to indicate the work in progress. When work is assigned, the initials of the analysts are stamped on the bottom edge of the card. As each analyst finishes his work, he crosses out his initials. Thus, an inspection of the card will tell im mediately the status of any job. After the analysis is completed, the Keysort card acts as an index to locate the corresponding analytical report. By suitable punches such in formation as the type of sample, the determinations made, the sender of the sample, and the date of receipt can be recorded on the Keysort card. The serial number of the sample
To take care of the first requirement a person or persons should be assigned to analytical research as their major job. As a minor part of this assign ment the person may be called upon occasionally to analyze unusual samples for which standardized methods are not available. A long range, continuing program of research should be planned for this unit. It should have as its broad objective the supplying of the analytical laboratory with the most up-to-date information on methods. For the second type of research requirement where a specific difficulty in carrying out an assignment has been encountered, it is good practice to assign a short term research proj ect to the analytical chemist who has encountered the difficulty. This per son will be most familiar with the problem and may have specialized skills which will have to be used in solving it. It should also stimulate the interest of the analyst to be able to follow through and work out a solu tion to his own problem. Ideas for research objectives should be solicited from all members of the staff and should be listed for review when time becomes available for undertaking a research assignment.
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V O L U M E 2 7, NO. 12, D E C E M B E R
1955
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